HRID53476

反应详情

EQUATION

反应方程式

HRID 53476 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3'-Amino-3'-deoxyadenosine 5'-triphosphate (15 mg, 26 mmol) and potassium carbonate (21 mg, 0.13 mmol) were dissolved in 2 ml of water. Sodium sulfosuccinimidyl acetate (36 mg, 0.13 mmol; Pierce Chemical, Rockford, Ill.) in 0.2 ml of dimethylsulfoxide (DMSO) was added at 0° C., and the reaction was allowed to proceed at room temperature for twenty-four hours. The product was purified by repeated injections on HPLC using a Synchropak RP-100 column (1×25 cm) applying a linear gradient of acetonitrile 5-22% TEAA (0.85 %/min, flow rate 3 ml/min, t=8.5 min). The appropriate fractions were collected and lyophilized to dryness. The product was obtained as a triethylammonium salt (8.5 mg, 39 %). UV: lmax =259 nm. High resolution MS for C12H18N6O13P3 : calcd. 547. 0145, found 547.0170 (MH3-).

WORKUP

后处理

  1. waitto proceed at room temperature for twenty-four hours
  2. customThe product was purified
  3. customa linear gradient of acetonitrile 5-22% TEAA (0.85 %/min, flow rate 3 ml/min, t=8.5 min)
  4. customThe appropriate fractions were collected